Thermo Scientific Orion AQUAfast Powder and Tablet Reagent Chemistry User Guide

Transcription

1 Thermo Scientific Orion AQUAfast Powder and Tablet Reagent Chemistry User Guide for use with AquaMate 7000 Vis and AquaMate 8000 UV-Vis Spectrophotometers

2 2012 Thermo Fisher Scientific Inc. All rights reserved. All trademarks are the property of Thermo Fisher Scientific Inc. and its subsidiaries.

3 Table of Contents Chapter 1 Overview... 1 Table 1: Orion AQUAfast Power and Tablet Reagent Chemistries... 2 Chapter 2 Reagent Chemistry Instructions... 4 Recommendations for Avoiding Measurement Errors... 4 Loading and Running a Water Analysis Method on the Spectrophotometer... 5 Loading a Test Method from the USB Stick to the AquaMate Instrument... 5 Running a Test Method from the USB Stick... 8 Running a Test Method from the AquaMate Instrument Library... 8 Running a Test Method from the AquaMate SmartStart Menu... 8 Using the One Point Adjustment Calibration Feature... 9 Using the Reverse Color Feature AC2002 Alkalinity-M (Alkalinity to ph 4.3), Acid/Indicator Method, Tablet Test Procedure AC3002P Alkalinity-P (Alkalinity to ph 8.2), Acid/Indicator Method, Tablet Test Procedure AC2027 Aluminum, Eriochrome Cyanine R Method, Tablet Test Procedure AC4P27 Aluminum, Eriochrome Cyanine R Method, Powder & Liquid Test Procedure AC2012 Ammonia as Nitrogen (N), Indophenole/Phenate Method, Tablet Test Procedure AC4P12 Ammonia as Nitrogen (N), Salicylate Method, Powder Test Procedure ACR011 Ammonia as Nitrogen (N), HR, Salicylate Method, Reaction Tube Test Procedure ACR012 Ammonia as Nitrogen (N), LR, Salicylate Method, Reaction Tube Test Procedure AC2035 Bromine, DPD Method, Tablet Test Procedure AC2017 Chloride, Silver Nitrate/Turbidity Method, Tablet Test Procedure AC2070 Chlorine, Free & Total, DPD Method, Tablet Test Procedure AC2071 Chlorine, Free, DPD Method, Tablet Test Procedure AC2072 Chlorine, Total, DPD Method, Tablet Test Procedure AC3072 Chlorine, Total, High Range, KI / Acid Method, Tablet Test Procedure AC4P71 Chlorine, Free, DPD Method, Powder Test Procedure AC4P72 Chlorine, Total, DPD Method, Powder Test Procedure AC2099 Chlorine Dioxide, DPD Method, Tablet Test Procedure CODL00 COD, Low Range, Dichromate Reactor Digestion Method, Digestion Tube Test Procedure CODH00 COD, Mid Range, Dichromate Reactor Digestion Method, Digestion Tube Test Procedure CODHP0 COD, High Range, Dichromate Reactor Digestion Method, Digestion Tube Test Procedure.. 35 AC2029 Copper, Free & Total, Biquinoline Method, Tablet Test Procedure AC2065 Copper, Zincon Method, Tablet Test Procedure AC4P29 Copper, Free, Bicinchoninate Method, Powder Test Procedure AC2098 Cyanuric Acid, Melamine Method, Tablet Test Procedure... 39

4 AC2009 Fluoride, SPADNS Kit Method, Liquid Test Procedure AC3032T Hardness, Total, Low Range, Metallphthalein Method, Tablet Test Procedure AC3032T Hardness, Total, High Range, Metallphthalein Method, Tablet Test Procedure AC2030 Hydrazine, Dimethylamino-benzaldehyde Method, Powder Test Procedure Iron Digestion Method AC2078 Iron, Low Range, III, Soluble, TPTZ Method, Tablet Test Procedure AC4P78 Iron, II & III, Soluble, 1,10-Phenanthroline Method, Powder Test Procedure AC4P79 Iron, Total, TPTZ Method, Powder Test Procedure AC2055 Manganese, Formaldoxime Method, Tablet Test Procedure AC4P54 Manganese, Low Range, PAN Method, Powder & Liquid Test Procedure AC4P55 Manganese, High Range, Periodate Oxidation Method, Powder Test Procedure AC4P42 Molybdate / Molybdenum, Mercaptoacetic Acid Method, Powder Test Procedure ACR007 Nitrate as Nitrogen (N), Chromotropic Acid Method, Reaction Tube Test Procedure AC2046 Nitrite as Nitrogen (N), Diazotization (Azo) Method, Tablet Test Procedure AC4P46 Nitrite as Nitrogen (N), Low Range, Diazotization (Azo) Method, Powder Test Procedure ACD004 Nitrogen, Total, Low Range, Persulfate Digestion Method, Digestion Tube Test Procedure ACD007 Nitrogen, Total, High Range, Persulfate Digestion Method, Digestion Tube Test Procedure.. 58 AC2048 Ozone, Indigo Blue, Tablet Test Procedure AC2001 ph, Phenol Red Method, Tablet Test Procedure AC3001 ph, Phenol Red Method, Liquid Test Procedure AC2095 Phosphate, Ortho, Low Range, Phosphomolybdic Acid/Ascorbic acid Method, Tablet Test Procedure AC2096 Phosphate, Ortho, High Range, Vanadomolybdate Method, Tablet Test Procedure AC4P95 Phosphate, Ortho, Ascorbic Acid Method, Powder Test Procedure ACD095 Phosphate as Phosphorous (P), Total, Persulfate Digestion/Ascorbic Acid Method, Digestion Tube Test Procedure ACD095AH Phosphate as Phosphorous (P), Acid Hydrolyzable, Acid Digestion/Ascorbic Acid Method, Digestion Tube Test Procedure ACR095 Phosphate, Ortho, Ascorbic Acid Method, Reaction Tube Test Procedure AC2060 Silica, Silicomolybdate Method, Tablet Test Procedure AC2061 Silica, Silicomolybdate Method with Phosphate Removal, Tablet Test Procedure AC4P60 Silica, High Range, Silicomolybdate Method, Powder Test Procedure AC4P82 Sulfate, Barium Sulfate/Turbidity Method, Powder Test Procedure AC2016 Sulfide, Methylene Blue Method, Tablet Test Procedure AC2065 Zinc, Zincon Method, Tablet Test Procedure... 78

5 Chapter 1 Overview Thermo Scientific Orion AquaMate 8000 UV-Vis and AquaMate 7000 Vis spectrophotometers include a USB memory stick that contains over 260 preprogrammed methods for use with Orion AQUAfast, Merck and CHEMetrics reagent chemistries. Preprogrammed methods provide values for the test parameters required to run specific reagent chemistries on the instrument, including wavelength, cell path length, concentration factors/curves and measurement unit. All preprogrammed methods are stored on the USB memory stick, so operators can select and load only the methods needed for their applications. Up to 90 methods can be stored on the AquaMate spectrophotometer and stored methods can be added or removed as needed. AquaMate spectrophotometers allow a one point adjustment on any preprogrammed method using a known standard to correct for variations in batch to batch reagent chemistries. Operators can also modify preprogrammed methods or create their own custom methods, so additional parameters and test methods can be added at any time. The following instructions are for using Orion AQUAfast reagent chemistries with the AquaMate spectrophotometer. Preprogrammed methods use a specific vial size (path length) in the formula, and the vial size specified in these instructions must be used for accurate analysis. The majority of AQUAfast reagent methods use a 24mm round vial, Cat. No. AC2V24. Other vial sizes are noted in the individual reagent chemistry instructions. Use the information in the following table to identify method names on the USB memory stick and the test parameters associated with each method. This information is also included in the Thermo Scientific AquaMate Master Methods List available on the user guide CD or on our website at Page 1

6 Table 1: Orion AQUAfast Power and Tablet Reagent Chemistries Parameter Reagent Part # Method Name Description Reagent Type Alkalinity AC2002 AC2002 Alkalinity-M, Acid/Indicator Method Tablet Alkalinity AC3002P AC3002P Alkalinity-P, Acid/Indicator Method Tablet Aluminum AC2027 AC2027 Aluminum, Eriochrome Cyanine R Method Tablet Aluminum AC4P27 AC4P27 Aluminum, Eriochrome Cyanine R Method Powder, Liquid Ammonia AC2012 AC2012 Ammonia as Nitrogen (N), Indophenole/Phenate Method Tablet Ammonia AC4P12 AC4P12 Ammonia as Nitrogen (N), Salicylate Method Powder Ammonia ACR011 ACR011 Ammonia ACR012 ACR012 Ammonia as Nitrogen (N), High Range, Salicylate Method Ammonia as Nitrogen (N), Low Range, Salicylate Method Reaction Tube Reaction Tube Bromine AC2035 AC Bromine, DPD Method Tablet Chloride AC2017 AC2017 Chloride, Silver Nitrate/Turbidity Method Tablet Chlorine AC2070 AC Chlorine, Free & Total, DPD Method Tablet Chlorine AC2071 AC Chlorine, Free, DPD Method Tablet Chlorine AC2072 AC Chlorine, Total, DPD Method Tablet Chlorine AC3072 AC3072 Chlorine, Total, High Range, KI / Acid Method Tablet Chlorine AC4P71 AC4P71 Chlorine, Free, DPD Method Powder Chlorine AC4P72 AC4P72 Chlorine, Total, DPD Method Powder Chlorine Dioxide AC2099 AC Chlorine Dioxide, DPD Method Tablet COD CODL00 CODL00 COD CODH00 CODH00 COD CODHP0 CODHP0 COD, Low Range, Dichromate Reactor Digestion Method COD, Mid Range, Dichromate Reactor Digestion Method COD, High Range, Dichromate Reactor Digestion Method Digestion Tube Digestion Tube Digestion Tube Copper AC2029 AC Copper, Free & Total, Biquinoline Method Tablet Copper AC2065 AC2065 Copper, Zincon Method Tablet Copper AC4P29 AC4P29 Copper, Free, Bicinchoninate Method Powder Cyanuric Acid AC2098 AC2098 Cyanuric Acid, Melamine Method Tablet Fluoride AC2009 AC2009 Fluoride, SPADNS Kit Method Liquid Hardness AC3032T AC3032TL Hardness, Total, Low Range, Metallphthalein Method Tablet Hardness AC3032T AC3032TH Hardness, Total, High Range, Metallphthalein Method Tablet Page 2

7 Hydrazine AC2030 AC2030 Hydrazine, Dimethylamino-benzaldehyde Method Powder Iron AC2078 AC Iron, Low Range, III, Soluble, TPTZ Method Tablet Iron AC4P78 AC4P78 Iron, II & III, Soluble, 1,10-Phenanthroline Method Powder Iron AC4P79 AC4P79 Iron, Total, TPTZ Method Powder Manganese AC2055 AC2055 Manganese, Formaldoxime Method Tablet Manganese AC4P54 AC4P54 Manganese, Low Range, PAN Method Manganese AC4P55 AC4P55 Molybdate / Molybdenum AC4P42 AC4P42 Manganese, High Range, Periodate Oxidation Method Molybdate / Molybdenum, Mercaptoacetic Acid Method Powder, Liquid Powder Powder Nitrate ACR007 ACR007 Nitrate as Nitrogen (N), Chromotropic Acid Method Reaction Tube Nitrite AC2046 AC2046 Nitrite as Nitrogen (N), Diazotization (Azo) Method Tablet Nitrite AC4P46 AC4P46 Nitrite as Nitrogen (N), Low Range, Diazotization (Azo) Method Powder Nitrogen, Total Nitrogen, Total ACD004 ACD007 ACD004 ACD007 Nitrogen, Total, Low Range, Persulfate Digestion Method Nitrogen, Total, High Range, Persulfate Digestion Method Digestion Tube Digestion Tube Ozone AC2048 AC Ozone, Indigo Blue Method Tablet ph AC2001 AC2001 ph, Phenol Red Method Tablet ph AC3001 AC3001 ph, Phenol Red Method Liquid Phosphate AC2095 AC2095 Phosphate, Low Range, Phosphomolybdic Acid/Ascorbic Acid Method Tablet Phosphate AC2096 AC2096 Phosphate, High Range, Vanadomolybdate Method Tablet Phosphate AC4P95 AC4P95 Phosphate, Ortho, Ascorbic Acid Method Powder Phosphate ACD095 ACD095 Phosphate ACD095AH ACD095AH Phosphate as Phosphorous (P), Total, Persulfate Digestion/Ascorbic Acid Method Phosphate as Phosphorous (P), Acid Hydrolyzable, Acid Digestion/Ascorbic Acid Method Phosphate ACR095 ACR095 Phosphate, Ortho, Ascorbic Acid Method Digestion Tube Digestion Tube Reaction Tube Silica AC2060 AC2060 Silica, Silicomolybdate Method Tablet Silica AC2061 AC2061 Silica, Silicomolybdate Method with Phosphate Removal Tablet Silica AC4P60 AC4P60 Silica, High Range, Silicomolybdate Method Powder Sulfate AC4P82 AC4P82 Sulfate, Barium Sulfate/Turbidity Method Powder Sulfide AC2016 AC2016 Sulfide, Methylene Blue Method Tablet Zinc AC2065 AC2065 Zinc, Zincon Method Tablet Page 3

8 Chapter 2 Reagent Chemistry Instructions The measurement ranges specified in the following test procedures are provided by the chemistry manufacturer and are based on standard solutions measured under ideal conditions. These ranges may vary due to the type of sample being measured, since various interferences can have a major influence on the accuracy of the method. Due to the fact that each sample is different, the only way to check the tolerance (precision) is the Standard Additions Method. According to this method, first the original sample is tested. Then further samples (2 to 4) are taken and small amounts of a standard solution are added, and further results are obtained. The amounts added range from approximately half, up to double the amount present in the sample itself. These supplementary results make it possible to estimate the actual concentration of the original sample by comparison. Test methods and ranges are subject to change without notice. For a list of the most up-to-date test methods, visit Recommendations for Avoiding Measurement Errors Thoroughly clean vials, caps and stir rods after each analysis in order to prevent carry-over errors. Even minute reagent residues lead to incorrect measurements. Ensure that the outer walls of the vials are dry and clean before performing the analysis. Fingerprints or water droplets on the light entry surfaces of the vials lead to incorrect measurements. Blank and measurement procedures should be performed using the same vial whenever possible, since different vials can possess slightly different tolerances. Always take all readings with capped vials. Bubbles on the inside walls of the vial can lead to incorrect measurements. To prevent this, cap the vial and remove the bubbles by swirling the vial before performing the test. Always add the reagent to the sample straight from the foil. The reagent should never touch fingers or hands. Major temperature differentials between the instrument and environment can lead to incorrect measurements - i.e. due to the formation of condensate in the area of the lens or on the vial. Specified tolerances at T = 20 C. For the best results, use a pipette to measure and add samples to vials or beakers. Page 4

9 Loading and Running a Water Analysis Method on the Spectrophotometer The USB memory stick included with the AquaMate spectrophotometers contains over 260 preprogrammed methods for use with Orion AQUAfast, Merck and CHEMetrics reagent chemistries. Methods can be accessed directly from the USB memory stick when connected to the AquaMate spectrophotometer or up to 90 methods can be stored on the instrument for quick and easy access. The USB memory stick contains four folders: Thermo, Orion, Merck and CHEMetrics. The Thermo folder is empty and all methods to be loaded on the AquaMate spectrophotometer need to be copied to the Thermo folder. The Orion, Merck and CHEMetrics folders contain preprogrammed methods specific to that manufacturer. Information for methods in the Orion folder can be found in this user guide and the Thermo Scientific Orion AquaMate Master Methods List document. Information for methods in the Merck and CHEMetrics folders can be found in the Thermo Scientific Orion AquaMate Master Methods List document and on the manufacturer s website. Recommendation: A copy of the methods on the USB memory stick should be saved to a computer or other data source in case the USB memory stick is accidentally deleted or otherwise corrupted. Loading a Test Method from the USB Stick to the AquaMate Instrument 1. Access the USB memory stick using a computer. 2. Copy the desired test method(s) from the Orion, Merck and/or CHEMetrics folders to the Thermo folder. 3. Remove the USB memory stick from the computer and insert it into the USB port on the front of the AquaMate spectrophotometer. 4. When the AquaMate spectrophotometer is first powered on, it will display the initial measurement screen. Press the Test key to access the test types. Page 5

10 5. Press the / keys to highlight Water Analysis and press the Enter key. 6. Press the Stored Tests function key. 7. Press the / keys to highlight Load test from USB drive and press the Enter key. 8. Press the / keys to highlight the test method to be loaded and press the Load Test function key. 9. Press the Save Test function key. Page 6

11 10. Press the / keys to highlight Save as an internal test and press the Enter key. 11. Press the Accept Name function key. 12. Press the / keys to highlight Include as a SmartStart test or Do not include as a SmartStart test and press the Enter key. 13. Press the Run Test function key to begin using the test method. Refer to the specific reagent chemistry section for detailed instructions. Page 7

12 Running a Test Method from the USB Stick 1. Make sure the test method to be run is in the Thermo folder on the USB stick and the USB stick is connected to the USB port on the front of the AquaMate spectrophotometer. 2. From the initial measurement screen, press the Test key to access the test types. 3. Press the / keys to highlight Water Analysis and press the Enter key. 4. Press the Stored Tests function key. 5. Press the / keys to highlight Load test from USB drive and press the Enter key. 6. Press the / keys to highlight the appropriate test method and press the Load Test function key. 7. Press the Run Test function key. Running a Test Method from the AquaMate Instrument Library 1. From the initial measurement screen, press the Test key to access the test types. 2. Press the / keys to highlight Water Analysis and press the Enter key. 3. Press the Stored Tests function key. 4. Press the / keys to highlight Load internal test and press the Enter key. 5. Press the / keys to highlight the appropriate test method and press the Load Test function key. 6. Press the Run Test function key. Running a Test Method from the AquaMate SmartStart Menu 1. From the initial measurement screen, press the Test key to access the test types. 2. Press the SmartStart function key. 3. Press the / keys to highlight the appropriate test method and press the Load Test function key. 4. Press the Run Test function key. Page 8

13 Using the One Point Adjustment Calibration Feature Use the one point adjustment feature prior to running a preprogrammed test method to ensure accurate measurements. This procedure is recommended each time a new batch of reagents are used to account for variations in batch-to-batch reagent composition and other factors that affect the accuracy of a method with a fixed calibration curve. When the one point adjustment feature is off, no adjustment is applied when running the test and test results are calculated exactly according to the preprogrammed equation. 1. Load the test method in the Water Analysis test menu. 2. If the 1pt Adjust parameter is set to Off, press the / keys to highlight 1pt Adjust and press the Enter key to set the parameter to On. 3. Prepare a blank, reagent blank (reverse color methods only) and calibration standard with a known concentration within the method range and near the expected sample concentration. Refer to the specific reagent chemistry section for detailed instructions. 4. Press the Calculate 1pt Adjust function key. 5. Use the numeric keypad to enter the concentration of the standard and press the Enter key. 6. Wipe the exterior of the blank vial and place the blank vial into the holder in the sample chamber. Close the sample chamber door. 7. Press the Measure Blank function key. 8. Open the sample chamber door and remove the vial from the sample chamber. 9. For reverse color methods only: a. Wipe the exterior of the reagent blank vial and place the reagent blank vial into the holder in the sample chamber. Close the sample chamber door. b. Press the Measure Rgnt Blank function key. c. Open the sample chamber door and remove the vial from the sample chamber. 10. Wipe the exterior of the standard vial and place the standard vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Standard function key. 12. Open the sample chamber door and remove the vial from the sample chamber. Page 9

14 13. The display will show the standard concentration that was entered in step 5, the measured concentration without a correction and the calculated adjustment correction factor. 14. Press the Accept function key if the calculated adjustment correction factor is acceptable. Typically a correction factor of 0.7 to 1.3 (within 30%) is acceptable. 15. To save the adjustment correction factor to the test method, press the Save Test function key and overwrite the existing test method or save as a new test method. 16. Press the Run Test function key. When running a test with an adjustment correction factor in use, the display will show (1pt Adj) next to the test name. Using the Reverse Color Feature Reverse color methods use a reagent that, when prepared with samples, deceases in color as the concentration of the species being measured in the samples increases. Reverse color methods require the use of both a blank and a reagent blank. The blank is a clear solution (deionized water) with zero absorbance. The reagent blank is a mixture of the reagent and deionized water (or initial reagent and sample, as in the zinc by zincon method) and provides a zero concentration point with the darkest color (highest absorbance). The color of samples prepared with the reagent will decrease as the concentration increases. The following provides an overview how to perform a reverse color method. 1. Load and run the method. The Reverse Color parameter should be set to On for the method. 2. Fill a vial with deionized water. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add the reagent(s) to the vial. Close the vial tightly with the cap and mix the contents. Wipe the exterior of the vial. 7. Place the vial into the holder in the sample chamber. Close the sample chamber door. 8. Press the Measure Rgnt Blank function key to measure the reagent blank. 9. Open the sample chamber door and remove the vial from the sample chamber. 10. Empty and rinse the vial and then fill the vial with sample. Add the reagent(s) to the vial. Close the vial tightly with the cap and mix the contents. Wipe the exterior of the vial. 11. Place the vial into the holder in the sample chamber. Close the sample chamber door. 12. Press the Measure Sample function key to display the results. Page 10

15 AC2002 Alkalinity-M (Alkalinity to ph 4.3), Acid/Indicator Method, Tablet Test Procedure mg/l CaCO 3 1. Load and run the AC2002 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Alka-M Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 8. Place the vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Sample function key to display the result in mg/l total alkalinity. The terms total alkalinity, alkalinity-m, m-value and alkalinity to ph 4.3 are identical. For accurate results exactly 10 ml of water sample must be taken for the test. Page 11

16 AC3002P Alkalinity-P (Alkalinity to ph 8.2), Acid/Indicator Method, Tablet Test Procedure mg/l CaCO 3 1. Load and run the AC3002P method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Alka-P Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 8. Place the vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Sample function key to display the result in mg/l total alkalinity. Notes The terms alkalinity-p, p-value and alkalinity to ph 8.2 are identical. For accurate test results exactly 10 ml of water sample must be taken for the test. This method was developed from a volumetric procedure for the determination of alkalinity-p. Due to undefined conditions, the deviations from the standardized method may be greater. Page 12

17 AC2027 Aluminum, Eriochrome Cyanine R Method, Tablet Test Procedure mg/l Al 1. Load and run the AC2027 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Aluminum No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod and mix well to dissolve the tablet completely. 7. Add one Aluminum No. 2 Tablet straight from the foil to the same vial. Crush the tablet with a clean stir rod and mix well to dissolve the tablet completely. 8. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 9. Wait for a reaction period of 5 minutes. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l aluminum. Before use, clean the vials and the measuring beaker with hydrochloric acid (approximately 20%). Rinse them thoroughly with deionized water. To get accurate results the sample temperature must be between 20 C and 25 C. A low test result may be given in the presence of fluorides and polyphosphates. The effect of this is generally insignificant unless the water has fluoride added artificially. Page 13

18 AC4P27 Aluminum, Eriochrome Cyanine R Method, Powder & Liquid Test Procedure mg/l Al 1. Load and run the AC4P27 method. 2. Use two clean AQUAfast 24mm round vials, Cat. No. AC2V24, and mark one as the blank. 3. Pour 20 ml of sample into a 100 ml beaker. 4. Add the contents of one Aluminum ECR F20 Powder Pack straight from the foil to the sample in the beaker. Dissolve the powder using a clean stirring rod. 5. Wait for a reaction period of 30 seconds. 6. Add the contents of one Hexamine F20 Powder Pack straight from the foil to the same sample in the beaker. Dissolve the powder using a clean stirring rod. 7. Add 1 drop of Aluminum ECR Masking Reagent in the vial marked as blank. Add 10 ml of the prepared sample to the same vial (this is the blank vial). 8. Add the remaining 10 ml of the prepared sample to the second vial (this is the sample vial). 9. Close the vials tightly with the caps and swirl or invert several times to mix the contents. Wipe the exteriors of the vials. 10. Wait for a reaction period of 5 minutes. 11. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 12. Press the Measure Blank function key to measure the blank. 13. Open the sample chamber door. Remove the blank vial from the holder. 14. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 15. Press the Measure Sample function key to display the result in mg/l aluminum. Before use, clean the vials and the measuring beaker with hydrochloric acid (approximately 20%). Rinse them thoroughly with deionized water. To get accurate results the sample temperature must be between 20 C and 25 C. A low test result may be given in the presence of fluorides and polyphosphates. The effect of this is generally insignificant unless the water has fluoride added artificially. Page 14

19 AC2012 Ammonia as Nitrogen (N), Indophenole/Phenate Method, Tablet Test Procedure mg/l N 1. Load and run the AC2012 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Ammonia No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Add one Ammonia No. 2 Tablet straight from the foil to the same sample in the vial. Crush the tablet with a clean stir rod. 8. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 9. Wait for a reaction period of 10 minutes. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l ammonia as N. The tablets must be added in the correct sequence. The Ammonia No. 1 Tablet will only dissolve completely after the Ammonia No. 2 Tablet has been added. The temperature of the sample is important for full color development. At a temperature below 20 C the reaction period is 15 minutes. Sea water samples: Ammonia conditioning reagent is required when testing sea water or brackish water samples to prevent precipitation of salts. Fill the test tube with the sample to the 10 ml mark and add one level spoonful of Conditioning Powder. Mix to dissolve and then continue as described in the test instructions. Page 15

20 AC4P12 Ammonia as Nitrogen (N), Salicylate Method, Powder Test Procedure mg/l N 1. Load and run the AC4P12 method. 2. Use two clean AQUAfast 24mm round vials, Cat. No. AC2V Pour 10 ml of deionized water into the first vial (this is the blank vial). 4. Pour 10 ml of sample into the second vial (this is the sample vial). 5. Add the contents of one Ammonia Salicylate F10 Powder Pack straight from the foil to each vial. Close the vials tightly with the caps and swirl or invert several times to mix the contents. 6. Wait for a reaction period of 3 minutes. 7. Add the contents of one Ammonia Cyanurate F10 Powder Pack straight from the foil to each vial. Close the vials tightly with the caps and swirl or invert several times to mix the contents. Wipe the exteriors of the vials. 8. Wait for a reaction period of 15 minutes. 9. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Blank function key to measure the blank. 11. Open the sample chamber door. Remove the blank vial from the holder. 12. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 13. Press the Measure Sample function key to display the result in mg/l ammonia as N. Extremely basic or acidic water samples should be adjusted with 0.5 mol/l (1 N) sulfuric acid solution or 1 mol/l (1 N) sodium hydroxide solution to ph 7. Interferences: Interference Interference Levels and Treatments Calcium Greater than 1000 mg/l CaCO 3 Iron Interferes at all levels. To correct, determine the concentration of iron in the sample by performing a total iron test. Add the same iron concentration to the deionized water (step 3). Iron will be blanked out successfully. Magnesium Greater than 6000 mg/l CaCO 3 Nitrate Greater than 100 mg/l NO 3 -N Nitrite Greater than 12 mg/l NO 2 -N Phosphate Greater than 100 mg/l PO 4 -P Sulfate Greater than 300 mg/l SO 4 Sulfide Intensifies the color Glycine, Hydrazine, Color, Turbidity Less common interferences such as hydrazine and glycine will cause intensified colors in the prepared sample. Turbidity and color will give erroneous high values. Samples with severe interferences require distillation. Page 16

21 ACR011 Ammonia as Nitrogen (N), HR, Salicylate Method, Reaction Tube Test Procedure 1 50 mg/l N 1. Load and run the ACR011 method. 2. Open one white capped 16mm reaction vial and add 0.1 ml of deionized water (this is the blank). 3. Open a second white capped 16mm reaction vial and add 0.1 ml of sample (this is the sample). 4. Add the contents of one Ammonia Salicylate F5 Powder Pack straight from the foil to each vial. 5. Add the contents of one Ammonia Cyanurate F5 Powder Pack straight from the foil to each vial. 6. Close the vials tightly with the caps and swirl or invert several times to mix the contents. Wipe the exteriors of the vials. 7. Wait for a reaction period of 20 minutes. 8. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Blank function key to measure the blank. 10. Open the sample chamber door. Remove the blank vial from the holder. 11. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 12. Press the Measure Sample function key to display the result in mg/l ammonia as N. Strong alkaline or acidic water samples must be adjusted to approximately ph 7 before analysis (use 1 mol/l hydrochloric acid or 1 mol/l sodium hydroxide). If chlorine is known to be present, add one drop of 0.1 mol/l sodium thiosulfate for each 0.3 mg/l Cl 2 in a one liter water sample. Iron interferes with the test. The interferences will be eliminated as follows: Determine the amount of total iron present in the water sample. To produce the blank add an iron standard solution with the same iron concentration to the vial (point 1) instead of deionized water Page 17

22 ACR012 Ammonia as Nitrogen (N), LR, Salicylate Method, Reaction Tube Test Procedure mg/l N 1. Load and run the ACR012 method. 2. Open one white capped 16mm reaction vial and add 2 ml of deionized water (this is the blank). 3. Open a second white capped 16mm reaction vial and add 2 ml of sample (this is the sample). 4. Add the contents of one Ammonia Salicylate F5 Powder Pack straight from the foil to each vial. 5. Close the vials tightly with the caps and swirl or invert several times to mix the contents. Wipe the exteriors of the vials. 6. Wait for a reaction period of 20 minutes. 7. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 8. Press the Measure Blank function key to measure the blank. 9. Open the sample chamber door. Remove the blank vial from the holder. 10. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l ammonia as N. Strong alkaline or acidic water samples must be adjusted to approximately ph 7 before analysis (use 1 mol/l hydrochloric acid or 1 mol/l sodium hydroxide). If chlorine is known to be present, add one drop of 0.1 mol/l sodium thiosulfate for each 0.3 mg/l Cl 2 in a one liter water sample. Iron interferes with the test. The interferences will be eliminated as follows: Determine the amount of total iron present in the water sample. To produce the blank add an iron standard solution with the same iron concentration to the vial (point 1) instead of deionized water Page 18

23 AC2035 Bromine, DPD Method, Tablet Test Procedure mg/l Br 2 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Empty the vial, leaving a few drops of sample remaining in the vial. 7. Add one DPD No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 8. Add sample to the 10 ml mark on the vial. 9. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l bromine. Vial cleaning: As many household cleaners (i.e. dishwasher detergent) contain reducing substances, the subsequent determination of bromine may show lower results. To avoid any measurement errors, only use glassware free of chlorine demand. Preparation: Put all applicable glassware into sodium hypochlorite solution (0.1 g/l) for one hour and then rinse all glassware thoroughly with deionized water. Preparing the sample: When preparing the sample, the escape of bromine gases, i.e. by pipetting or shaking, must be avoided. The analysis must take place immediately after taking the sample. The DPD color development is carried out at a ph value of 6.2 to 6.5. The reagent tablet therefore contains a buffer for the ph adjustment. Strong alkaline or acidic water samples must be adjusted between ph 6 and ph 7 before the reagent is added (use 0.5 mol/l sulfuric acid or 1 mol/l sodium hydroxide). Exceeding the measuring range: Concentrations above 22 mg/l bromine can lead to results showing 0 mg/l. In this event, the water sample must be diluted with water free of bromine. 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated. Oxidizing agents such as chlorine or ozone interfere as they react in the same way as bromine. Page 19

24 AC2017 Chloride, Silver Nitrate/Turbidity Method, Tablet Test Procedure mg/l Cl 1. Load and run the AC2017 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Chloride T1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Add one Chloride T2 Tablet straight from the foil to the same vial. Crush the tablet with a clean stir rod. 8. Close the vial tightly with the cap and swirl gently until the tablet is dissolved. Wipe the exterior of the vial. 9. Wait for a reaction period of 2 minutes. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l chloride. Ensure that all particles of the tablet are dissolved chloride causes an extremely fine distributed turbidity with a milky appearance. Heavy shaking leads to bigger sized particles which can cause false readings. High concentrations of electrolytes and organic compounds have different effects on the precipitation reaction. Ions which also form deposits with silver nitrate in acidic media, such as bromides, iodides and thiocyanates, interfere with the analysis. Highly alkaline water should, if necessary, be neutralized using nitric acid before analysis. Page 20

25 AC2070 Chlorine, Free & Total, DPD Method, Tablet Test Procedure mg/l Cl 2 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Empty the vial, leaving a few drops of sample remaining in the vial. 7. Add one DPD No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 8. Add sample to the 10 ml mark on the vial. 9. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l free chlorine. 12. Open the sample chamber door and remove the vial from the sample chamber. 13. Add one DPD No. 3 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 14. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 15. Wait for a reaction period of 2 minutes. 16. Place the vial into the holder in the sample chamber. Close the sample chamber door. 17. Press the Measure Sample function key to display the result in mg/l total chlorine. Vial cleaning: As many household cleaners (i.e. dishwasher detergent) contain reducing substances, the subsequent determination of chlorine may show lower results. To avoid any measurement errors, only use glassware free of chlorine demand. Preparation: Put all applicable glassware into sodium hypochlorite solution (0.1 g/l) for one hour and then rinse all glassware thoroughly with deionized water. For individual testing of free and total chlorine, the use of different sets of glassware is recommended (EN ISO , 5.3). Preparing the sample: When preparing the sample, the escape of chlorine gases, i.e. by pipetting or shaking, must be avoided. The analysis must take place immediately after taking the sample. Page 21

26 The DPD color development is carried out at a ph value of 6.2 to 6.5. The reagents therefore contain a buffer for the ph adjustment. Strong alkaline or acidic water samples must be adjusted between ph 6 and ph 7 before the reagent is added (use 0.5 mol/l sulfuric acid or 1 mol/l sodium hydroxide). Exceeding the measuring range: Concentrations above 10 mg/l chlorine using tablets can lead to results showing 0 mg/l. In this event, the water sample must be diluted with water free of chlorine. 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated. Turbidity (can lead to errors): The use of the DPD No. 1 Tablet in samples with high calcium ion contents and/or high conductivity can lead to turbidity of the sample and therefore incorrect measurements. In this event, the reagent DPD No. 1 High Calcium Tablet should be used as an alternative. Even if turbidity does occur after the DPD No. 3 Tablet has been added, it can be prevented by using the DPD No. 1 High Calcium Tablet. It is not possible to give exact values, because the development of turbidity depends on the nature of the sample. Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine. Page 22

27 AC2071 Chlorine, Free, DPD Method, Tablet Test Procedure mg/l Cl 2 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Empty the vial, leaving a few drops of sample remaining in the vial. 7. Add one DPD No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 8. Add sample to the 10 ml mark on the vial. 9. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l free chlorine. Vial cleaning: As many household cleaners (i.e. dishwasher detergent) contain reducing substances, the subsequent determination of chlorine may show lower results. To avoid any measurement errors, only use glassware free of chlorine demand. Preparation: Put all applicable glassware into sodium hypochlorite solution (0.1 g/l) for one hour and then rinse all glassware thoroughly with deionized water. For individual testing of free and total chlorine, the use of different sets of glassware is recommended (EN ISO , 5.3). Preparing the sample: When preparing the sample, the escape of chlorine gases, i.e. by pipetting or shaking, must be avoided. The analysis must take place immediately after taking the sample. The DPD color development is carried out at a ph value of 6.2 to 6.5. The reagents therefore contain a buffer for the ph adjustment. Strong alkaline or acidic water samples must be adjusted between ph 6 and ph 7 before the reagent is added (use 0.5 mol/l sulfuric acid or 1 mol/l sodium hydroxide). Exceeding the measuring range: Concentrations above 10 mg/l chlorine using tablets can lead to results showing 0 mg/l. In this event, the water sample must be diluted with water free of chlorine. 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated. Turbidity (can lead to errors): The use of the DPD No. 1 Tablet in samples with high calcium ion contents and/or high conductivity can lead to turbidity of the sample and therefore incorrect Page 23

28 measurements. In this event, the reagent DPD No. 1 High Calcium Tablet should be used as an alternative. It is not possible to give exact values, because the development of turbidity depends on the nature of the sample. Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine. Page 24

29 AC2072 Chlorine, Total, DPD Method, Tablet Test Procedure mg/l Cl 2 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Empty the vial, leaving a few drops of sample remaining in the vial. 7. Add one DPD No. 1 Tablet and one DPD No. 3 Tablet straight from the foil to the vial. Crush the tablets with a clean stir rod. 8. Add sample to the 10 ml mark on the vial. 9. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 10. Wait for a reaction period of 2 minutes. 11. Place the vial into the holder in the sample chamber. Close the sample chamber door. 12. Press the Measure Sample function key to display the result in mg/l total chlorine. Vial cleaning: As many household cleaners (i.e. dishwasher detergent) contain reducing substances, the subsequent determination of chlorine may show lower results. To avoid any measurement errors, only use glassware free of chlorine demand. Preparation: Put all applicable glassware into sodium hypochlorite solution (0.1 g/l) for one hour and then rinse all glassware thoroughly with deionized water. For individual testing of free and total chlorine, the use of different sets of glassware is recommended (EN ISO , 5.3). Preparing the sample: When preparing the sample, the escape of chlorine gases, i.e. by pipetting or shaking, must be avoided. The analysis must take place immediately after taking the sample. The DPD color development is carried out at a ph value of 6.2 to 6.5. The reagents therefore contain a buffer for the ph adjustment. Strong alkaline or acidic water samples must be adjusted between ph 6 and ph 7 before the reagent is added (use 0.5 mol/l sulfuric acid or 1 mol/l sodium hydroxide). Exceeding the measuring range: Concentrations above 10 mg/l chlorine using tablets can lead to results showing 0 mg/l. In this event, the water sample must be diluted with water free of chlorine. 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated. Page 25

30 Turbidity (can lead to errors): The use of the DPD No. 1 Tablet in samples with high calcium ion contents and/or high conductivity can lead to turbidity of the sample and therefore incorrect measurements. In this event, the reagent DPD No. 1 High Calcium Tablet should be used as an alternative. Even if turbidity does occur after the DPD No. 3 Tablet has been added, it can be prevented by using the DPD No. 1 High Calcium Tablet. It is not possible to give exact values, because the development of turbidity depends on the nature of the sample. Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine. Page 26

31 AC3072 Chlorine, Total, High Range, KI / Acid Method, Tablet Test Procedure mg/l Cl 2 1. Load and run the AC3072 method. 2. Fill a clean AQUAfast 16 mm round vial, Cat. No. AC2V16, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Chlorine HR (KI) Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Add one Acidifying GP Tablet straight from the foil to the same vial. Crush the tablet with a clean stir rod. 8. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l chlorine. Oxidizing agents interfere as they react in the same way as chlorine. Page 27

32 AC4P71 Chlorine, Free, DPD Method, Powder Test Procedure mg/l Cl 2 1. Load and run the AC4P71 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Chlorine Free-DPD / F10 Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents (approximately 20 seconds). Wipe the exterior of the vial. 8. Place the vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Sample function key to display the result in mg/l free chlorine. Vial cleaning: As many household cleaners (i.e. dishwasher detergent) contain reducing substances, the subsequent determination of chlorine may show lower results. To avoid any measurement errors, only use glassware free of chlorine demand. Preparation: Put all applicable glassware into sodium hypochlorite solution (0.1 g/l) for one hour and then rinse all glassware thoroughly with deionized water. For individual testing of free and total chlorine, the use of different sets of glassware is recommended (EN ISO , 5.3). Preparing the sample: When preparing the sample, the escape of chlorine gases, i.e. by pipetting or shaking, must be avoided. The analysis must take place immediately after taking the sample. The DPD color development is carried out at a ph value of 6.2 to 6.5. The reagents therefore contain a buffer for the ph adjustment. Strong alkaline or acidic water samples must be adjusted between ph 6 and ph 7 before the reagent is added (use 0.5 mol/l sulfuric acid or 1 mol/l sodium hydroxide). Exceeding the measuring range: Concentrations above 2 mg/l chlorine using powder packs can lead to results showing 0 mg/l. In this event, the water sample must be diluted with water free of chlorine. 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated. Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine. Page 28

33 AC4P72 Chlorine, Total, DPD Method, Powder Test Procedure mg/l Cl 2 1. Load and run the AC4P72 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Chlorine Total-DPD / F10 Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents (approximately 20 seconds). Wipe the exterior of the vial. 8. Wait for a reaction period of 3 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l total chlorine. Vial cleaning: As many household cleaners (i.e. dishwasher detergent) contain reducing substances, the subsequent determination of chlorine may show lower results. To avoid any measurement errors, only use glassware free of chlorine demand. Preparation: Put all applicable glassware into sodium hypochlorite solution (0.1 g/l) for one hour and then rinse all glassware thoroughly with deionized water. For individual testing of free and total chlorine, the use of different sets of glassware is recommended (EN ISO , 5.3). Preparing the sample: When preparing the sample, the escape of chlorine gases, i.e. by pipetting or shaking, must be avoided. The analysis must take place immediately after taking the sample. The DPD color development is carried out at a ph value of 6.2 to 6.5. The reagents therefore contain a buffer for the ph adjustment. Strong alkaline or acidic water samples must be adjusted between ph 6 and ph 7 before the reagent is added (use 0.5 mol/l sulfuric acid or 1 mol/l sodium hydroxide). Exceeding the measuring range: Concentrations above 2 mg/l chlorine using powder packs can lead to results showing 0 mg/l. In this event, the water sample must be diluted with water free of chlorine. 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated. Oxidizing agents such as bromine or ozone interfere as they react in the same way as chlorine. Page 29

34 AC2099 Chlorine Dioxide, DPD Method, Tablet Test Procedure mg/l ClO 2 Chlorine Dioxide Measurement in Absence of Chlorine 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Empty the vial, leaving a few drops of sample remaining in the vial. 7. Add one DPD No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 8. Add sample to the 10 ml mark on the vial. 9. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l chlorine dioxide. Chlorine Dioxide Measurement in Presence of Chlorine 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Empty the vial, leaving a few drops of sample remaining in the vial. 7. Add one DPD No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 8. Fill a second clean AQUAfast 24mm round vial with 10 ml of sample. Add one Glycine Tablet straight from the foil to the vial. Crush the tablets with a clean stir rod. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. 9. Transfer the contents of the second vial into the first vial. 10. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 11. Place the vial into the holder in the sample chamber. Close the sample chamber door. Page 30

35 12. Press the Measure Sample function key to display the result in mg/l chlorine dioxide. Vial cleaning: As many household cleaners (i.e. dishwasher detergent) contain reducing substances, the subsequent determination of chlorine dioxide may show lower results. To avoid any measurement errors, only use glassware free of chlorine demand. Preparation: Put all applicable glassware into sodium hypochlorite solution (0.1 g/l) for one hour and then rinse all glassware thoroughly with deionized water. Preparing the sample: When preparing the sample, the escape of chlorine dioxide gases, i.e. by pipetting or shaking, must be avoided. The analysis must take place immediately after taking the sample. The DPD color development is carried out at a ph value of 6.2 to 6.5. The reagent tablet therefore contains a buffer for the ph adjustment. Strong alkaline or acidic water samples must be adjusted between ph 6 and ph 7 before the tablet is added (use 0.5 mol/l sulfuric acid or 1 mol/l sodium hydroxide). Exceeding the measuring range: Concentrations above 19 mg/l chlorine dioxide can lead to results showing 0 mg/l. In this event, the water sample must be diluted with water free of chlorine dioxide. 10 ml of the diluted sample should be mixed with the reagent and the measurement repeated. Oxidizing agents such as chlorine or ozone interfere as they react in the same way as chlorine dioxide. Page 31

36 CODL00 COD, Low Range, Dichromate Reactor Digestion Method, Digestion Tube Test Procedure mg/l O 2 1. Open one white capped 16mm COD reaction vial and add 2 ml of deionized water (this is the reagent blank). 2. Open a second white capped 16mm reaction vial and add 2 ml of sample (this is the sample). 3. Close the vials tightly with the caps and gently invert the vials several times to mix the contents. CAUTION: The vials will become hot during mixing. 4. Heat the vials for 120 minutes in the preheated reactor at a temperature of 150 C. 5. CAUTION: The vials will be hot. Remove the vials from the reactor and allow them to cool to 60 C or less. Gently invert the vials several times to mix the contents while still warm. Then allow the vials to cool to ambient temperature before measuring. Wipe the exteriors of the vials. 6. Load and run the CODL00 method. 7. Fill a clean AQUAfast 16mm round vial, Cat. No. AC2V16, with deionized water (this is the blank). Close the vial tightly with the cap. Wipe the exterior of the vial. 8. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Blank function key to measure the blank. 10. Open the sample chamber door. Remove the blank vial from the holder. 11. Place the reagent blank vial into the holder in the sample chamber. Close the sample chamber door. 12. Press the Measure Rgnt Blank function key to measure the reagent blank. 13. Open the sample chamber door. Remove the reagent blank vial from the holder. 14. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 15. Press the Measure Sample function key to display the result in mg/l COD. Reverse color methods use a reagent that, when prepared with samples, deceases in color as the concentration of the species being measured in the samples increases. Reverse color methods require the use of both a blank and a reagent blank. The blank is a clear solution (deionized water) with zero absorbance. The reagent blank is a mixture of the reagent and deionized water and provides a zero concentration point with the darkest color (highest absorbance). The color of samples prepared with the reagent will decrease as the concentration increases for this method. Run samples and blanks with the same batch of vials. The blank is stable when stored in the dark and can be used for further measurements with vials of the same batch. Page 32

37 Do not place the hot vials in the sample chamber. Cool the vials to room temperature for final measurements. Suspended solids in the vial lead to incorrect measurements. For this reason it is important to place the vials carefully in the sample chamber. The precipitate at the bottom of the sample should be not suspended. Clean the outside of the vials with a towel. Finger prints or other marks must be removed. Samples can be measured when the chloride content does not exceed 1000 mg/l. In exceptional cases, compounds contained in the water cannot be oxidized adequately, so results may be lower than reference methods. Page 33

38 CODH00 COD, Mid Range, Dichromate Reactor Digestion Method, Digestion Tube Test Procedure mg/l O 2 1. Open one white capped 16mm COD reaction vial and add 2 ml of deionized water (this is the blank). 2. Open a second white capped 16mm COD reaction vial and add 2 ml of sample (this is the sample). 3. Close the vial tightly with the cap and gently invert the vials several times to mix the contents. CAUTION: The vials will become hot during mixing. 4. Heat the vials for 120 minutes in the preheated reactor at a temperature of 150 C. 5. CAUTION: The vials will be hot. Remove the vials from the reactor and allow them to cool to 60 C or less. Gently invert the vials several times to mix the contents while still warm. Then allow the vials to cool to ambient temperature before measuring. Wipe the exteriors of the vials. 6. Load and run the CODH00 method. 7. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 8. Press the Measure Blank function key to measure the blank. 9. Open the sample chamber door. Remove the blank vial from the holder. 10. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l COD. Run samples and blanks with the same batch of vials. The blank is stable when stored in the dark and can be used for further measurements with vials of the same batch. Do not place the hot vials in the sample chamber. Cool the vials to room temperature for final measurements. Suspended solids in the vial lead to incorrect measurements. For this reason it is important to place the vials carefully in the sample chamber. The precipitate at the bottom of the sample should be not suspended. Clean the outside of the vials with a towel. Finger prints or other marks must be removed. Samples can be measured when the chloride content does not exceed 1000 mg/l. In exceptional cases, compounds contained in the water cannot be oxidized adequately, so results may be lower than reference methods. For samples under 100 mg/l COD it is recommended to repeat the test using the reaction tube test for COD LR. Page 34

39 CODHP0 COD, High Range, Dichromate Reactor Digestion Method, Digestion Tube Test Procedure mg/l O 2 1. Open one white capped 16mm COD reaction vial and add 0.2 ml of deionized water (this is the blank). 2. Open a second white capped 16mm COD reaction vial and add 0.2 ml of sample (this is the sample). 3. Close the vial tightly with the cap and gently invert the vials several times to mix the contents. CAUTION: The vials will become hot during mixing. 4. Heat the vials for 120 minutes in the preheated reactor at a temperature of 150 C. 5. CAUTION: The vials will be hot. Remove the vials from the reactor and allow them to cool to 60 C or less. Gently invert the vials several times to mix the contents while still warm. Then allow the vials to cool to ambient temperature before measuring. Wipe the exteriors of the vials. 6. Load and run the CODHP0 method. 7. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 8. Press the Measure Blank function key to measure the blank. 9. Open the sample chamber door. Remove the blank vial from the holder. 10. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l COD. Run samples and blanks with the same batch of vials. The blank is stable when stored in the dark and can be used for further measurements with vials of the same batch. Do not place the hot vials in the sample chamber. Cool the vials to room temperature for final measurements. Suspended solids in the vial lead to incorrect measurements. For this reason it is important to place the vials carefully in the sample chamber. The precipitate at the bottom of the sample should be not suspended. Clean the outside of the vials with a towel. Finger prints or other marks must be removed. Samples can be measured when the chloride content does not exceed 1000 mg/l. In exceptional cases, compounds contained in the water cannot be oxidized adequately, so results may be lower than reference methods. For samples under 1000 mg/l COD it is recommended to repeat the test using the reaction tube test for COD MR or for samples under 100 mg/l COD it is recommended to repeat the test using the reaction tube test for COD LR. Page 35

40 AC2029 Copper, Free & Total, Biquinoline Method, Tablet Test Procedure mg/l Cu 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Copper No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 8. Place the vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Sample function key to display the result in mg/l free copper. 10. Open the sample chamber door and remove the vial from the sample chamber. 11. Add one Copper No.2 Tablet straight from the foil to the same vial. Crush the tablet with a clean stir rod. 12. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial Press the Measure Sample function key to display the result in mg/l total copper. Page 36

41 AC2065 Copper, Zincon Method, Tablet Test Procedure mg/l Cu 1. Load and run the AC2065 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Copper / Zinc LR Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. 8. Wait for a reaction period of 5 minutes. 9. Add one EDTA Tablet straight from the foil to the same vial. Crush the tablet with a clean stir rod. 10. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 11. Place the vial into the holder in the sample chamber. Close the sample chamber door. 12. Press the Measure Sample function key to display the result in mg/l copper. The tablets must be added in the correct sequence. If the sample is zinc-free, it is not necessary to add the EDTA Tablet. Page 37

42 AC4P29 Copper, Free, Bicinchoninate Method, Powder Test Procedure mg/l Cu 1. Load and run the AC4P29 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Cu 1 F10 Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 8. Wait for a reaction period of 2 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l free copper. For determination of total copper digestion is required. Extremely acid water samples (ph 2 or less) must be adjusted between ph 4 and ph 6 before the reagent is added (with 8 mol/l potassium hydroxide solution KOH). Accuracy is not affected by undissolved powder. Interferences: Cyanide (CN - ) Cyanide prevents full color development. Add 0.2 ml formaldehyde to 10 ml water sample and wait for a reaction time of 4 minutes (cyanide is masked). After this perform test as described. Multiply the result by 1.02 to correct the sample dilution by formaldehyde. Silver (Ag + ) If turbidity remains and turns black, silver interference is likely. Add 10 drops of saturated potassium chloride solution to 75 ml of water sample. Filtrate through a fine filter. Use 10 ml of the filtered water sample to perform test. Page 38

43 AC2098 Cyanuric Acid, Melamine Method, Tablet Test Procedure 5 90 mg/l CyA 1. Load and run the AC2098 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Cyanuric Acid Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved (see notes below). Wipe the exterior of the vial. 8. Place the vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Sample function key to display the result in mg/l cyanuric acid. If cyanuric acid is present a cloudy solution will occur. Small single particles are not necessarily caused by cyanuric acid. Dissolve the tablet completely (swirl the vial for approximately 1 minute). Undissolved particles of the tablet can cause results that are too high. Exceeding the measurement range: samples with concentration above 90mg/L must be diluted with water free of cyanuric acid. 10 ml of the diluted sample should be tested as described above and the displayed results calculated using the dilution factor. Page 39

44 AC2009 Fluoride, SPADNS Kit Method, Liquid Test Procedure mg/l F 1. Load and run the AC2009 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with exactly 10 ml of deionized water. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add exactly 2 ml SPADNS Solution to the vial. CAUTION: The vial will be filled up to the top. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 8. Place the vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Rgnt Blank function key to measure the reagent blank. 10. Open the sample chamber door and remove the vial from the sample chamber. 11. Empty the vial, rinse the vial and cap several times and fill the vial with exactly 10 ml of sample. 12. Add exactly 2 ml SPADNS Solution to the vial. CAUTION: The vial will be filled up to the top. 13. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 14. Place the vial into the holder in the sample chamber. Close the sample chamber door. 15. Press the Measure Sample function key to display the result in mg/l fluoride. Reverse color methods use a reagent that, when prepared with samples, deceases in color as the concentration of the species being measured in the samples increases. Reverse color methods require the use of both a blank and a reagent blank. The blank is a clear solution (deionized water) with zero absorbance. The reagent blank is a mixture of the reagent and deionized water and provides a zero concentration point with the darkest color (highest absorbance). The color of samples prepared with the reagent will decrease as the concentration increases for this method. The same batch of SPADNS reagent solution must be used for testing (reagent blank and sample measurement) and one point calibration procedures. The one point calibration process needs to be performed for each new batch of SPADNS reagent solution (see Standard Methods 20 th ed., 1998, APHA, AWWA, WEF 4500 F - D, 4.a). During testing (blank, reagent blank and sample measurement) and one point calibration procedures the same vial should be used, as different vials may exhibit minor tolerances. The calibration solution and water samples should have the same temperature (+/- 1 C). Page 40

45 As the test result is highly dependent on exact sample and reagent volumes, the sample and reagent volumes should always be measured using a 10 ml or 2 ml volumetric pipette (class A). The accuracy of the test methods decreases above a level of 1.2 mg/l fluoride. Although the results are sufficiently accurate for most applications, even more exact results can be achieved by 1:1 dilution of the sample prior to use and subsequent multiplication of the result by 2. SPADNS reagent solution contains arsenite. Chlorine concentrations up to 5 mg/l do not interfere. Seawater and wastewater samples must be distilled. Page 41

46 AC3032T Hardness, Total, Low Range, Metallphthalein Method, Tablet Test Procedure 2 50 mg/l CaCO 3 1. Load and run the AC3032TL method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Hardcheck P Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 8. Wait for a reaction period of 5 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l total hardness. Strong alkaline or acidic water samples must be adjusted between ph 4 and ph 10 before the tablet is added (use 1 mol/l hydrochloric acid or 1 mol/l sodium hydroxide). Page 42

47 AC3032T Hardness, Total, High Range, Metallphthalein Method, Tablet Test Procedure mg/l CaCO 3 1. Load and run the AC3032TH method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 1 ml of sample and 9 ml of deionized water. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Hardcheck P Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 8. Wait for a reaction period of 5 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l total hardness. Strong alkaline or acidic water samples must be adjusted between ph 4 and ph 10 before the tablet is added (use 1 mol/l hydrochloric acid or 1 mol/l sodium hydroxide). Page 43

48 AC2030 Hydrazine, Dimethylamino-benzaldehyde Method, Powder Test Procedure mg/l N 2 H 4 1. Load and run the AC2030 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one gram (1 g) Hydrazine Powder to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 8. Wait for a reaction period of 10 minutes. 9. The slight turbidity that occurs when the reagent is added must be removed by filtration 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l hydrazine. If the water sample is cloudy, you must filter it before performing the blank measurement. The temperature of the water sample should not exceed 21 C. Using the Hydrazine spoon: 1 g is equivalent to one level spoon. Qualitative folded filter papers for medium precipitates are recommended. In order to check whether the reagent has aged (if it has been stored for a lengthy period), perform the test as described above using tap water. If the result is above the detection limit of 0.05 mg/l, you should only use the reagent with reservations as there may be a major deviation in results. Page 44

49 Iron Digestion Method Digestion procedure for the determination of total soluble and insoluble iron: 1. Add 1 ml of concentrated sulfuric acid to 100 ml water sample. Heat and boil for 10 minutes or until all particles are dissolved. After cooling down, the sample is set to a ph value of 3 to 6 by using ammonia solution. Refill with deionized water to the previous volume of 100 ml and mix well. 10 ml of this pre-treated solution is used for the following analysis. Perform as described by the selected test method. 2. Water which has been treated with organic compounds like corrosion inhibitors must be oxidized where necessary to break down the iron. Therefore add 1 ml concentrated sulfuric acid and 1 ml concentrated nitric acid to 100 ml water sample and boil to approximately half volume. After cooling down, proceed as described above. Page 45

50 AC2078 Iron, Low Range, III, Soluble, TPTZ Method, Tablet Test Procedure mg/l Fe 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Iron LR Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 8. Wait for a reaction period of 5 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l iron. This method determines the total dissolved iron as Fe 2+ and Fe 3+. The Iron (II) LR Tablet is used for differentiation, as described in the Iron Digestion Method section, instead of the Iron LR Tablet. For the determination of total dissolved and undissolved iron, digestion is required. An example is described in the Iron Digestion Method section. Page 46

51 AC4P78 Iron, II & III, Soluble, 1,10-Phenanthroline Method, Powder Test Procedure mg/l Fe 1. Load and run the AC4P78 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Ferro F10 Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 8. Wait for a reaction period of 3 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l iron. The reagent reacts with all soluble iron and most insoluble forms of iron in the water sample. Iron oxide requires prior digestion: use mild, vigorous or Digesdahl digestion. For an example of digestion with acid, refer to the Iron Digestion Method section. Very strong alkaline or acidic samples must be adjusted to a ph value between 3 and 5 before analysis. Accuracy is not affected by undissolved powder. Water samples containing visible rust should be allowed to react for at least five minutes. Page 47

52 AC4P79 Iron, Total, TPTZ Method, Powder Test Procedure mg/l Fe 1. Load and run the AC4P79 method. 2. Use two clean AQUAfast 24mm round vials, Cat. No. AC2V Pour 10 ml of deionized water into the first vial (this is the blank vial). 4. Pour 10 ml of sample into the second vial (this is the sample vial). 5. Add the contents of one Iron TPTZ F10 Powder Pack straight from the foil to each vial. Close the vials tightly with the caps and swirl or invert several times to mix the contents. Wipe the exteriors of the vials. 6. Wait for a reaction period of 3 minutes. 7. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 8. Press the Measure Blank function key to measure the blank. 9. Open the sample chamber door. Remove the blank vial from the holder. 10. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l iron. For determination of total Iron digestion is required. TPTZ reagent recovers most insoluble iron oxides without digestion. Rinse all glassware with 1:1 hydrochloric acid solution first and then rinse with deionized water to remove iron deposits that can cause slightly high results. Strong alkaline or acidic water samples must be adjusted between ph 3 and ph 8 before the reagent is added (use 0.5 mol/l sulfuric acid or 1 mol/l sodium hydroxide). Interferences: When interferences occur, color development is inhibited or a precipitate is formed. The values below refer to a standard with an iron concentration of 0.5 mg/l. The following substances do not interfere when present up to the levels given: Substance No Interference To Substance No Interference To Cadmium 4.0 mg/l Manganese 50 mg/l Chromium( 3+ ) 0.25 mg/l Mercury 0.4 mg/l Chromium ( 6+ ) 1.2 mg/l Molybdenum 4.0 mg/l Cobalt 0.05 mg/l Nickel 1.0 mg/l Copper 0.6 mg/l Nitrite Ion 0.8 mg/l Cyanide 2.8 mg/l Page 48

53 AC2055 Manganese, Formaldoxime Method, Tablet Test Procedure mg/l Mn 1. Load and run the AC2055 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Manganese LR 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Add one Manganese LR 2 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 8. Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved. Wipe the exterior of the vial. 9. Wait for a reaction period of 5 minutes. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l manganese. Page 49

54 AC4P54 Manganese, Low Range, PAN Method, Powder & Liquid Test Procedure mg/l Mn 1. Load and run the AC4P54 method. 2. Use two clean AQUAfast 24mm round vials, Cat. No. AC2V Pour 10 ml of deionized water into the first vial (this is the blank vial). 4. Pour 10 ml of sample into the second vial (this is the sample vial). 5. Add the contents of one Ascorbic Acid Powder Pack straight from the foil to each vial. Close the vials tightly with the caps and swirl or invert several times to mix the contents. 6. Add 15 drops of Alkaline Cyanide Reagent Solution to each vial. Add drops of the same size by holding the bottle vertically and squeezing slowly. Close the vials tightly with the caps and swirl or invert several times to mix the contents. 7. Add 21 drops of PAN Indicator Solution to each vial. Add drops of the same size by holding the bottle vertically and squeezing slowly. Close the vials tightly with the caps and swirl or invert several times to mix the contents. Wipe the exteriors of the vials. 8. Wait for a reaction period of 2 minutes. 9. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Blank function key to measure the blank. 11. Open the sample chamber door. Remove the blank vial from the holder. 12. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 13. Press the Measure Sample function key to display the result in mg/l manganese. Rinse all glassware with 1:1 nitric acid solution first and then rinse with deionized water. Water samples that contain more than 300 mg/l CaCO 3 hardness: after adding the Ascorbic Acid Powder Pack add additionally 10 drops of Rochelle Salt Solution. After addition of the Alkaline Cyanide Reagent Solution a cloudy or turbid solution may form in some water samples. The turbidity should disappear after the PAN Indicator Solution is added. Water samples containing more than 5 mg/l iron should be allowed to react for at least 10 minutes. Page 50

55 AC4P55 Manganese, High Range, Periodate Oxidation Method, Powder Test Procedure mg/l Mn 1. Load and run the AC4P55 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Citrat Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. 8. Add one Sodium Periodate Powder Pack straight from the foil to the vial. 9. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 10. Wait for a reaction period of 2 minutes. 11. Place the vial into the holder in the sample chamber. Close the sample chamber door. 12. Press the Measure Sample function key to display the result in mg/l manganese. This test is applicable for the determination of soluble manganese in water and wastewater. Highly buffered water samples or extreme ph values may exceed the buffering capacity of the reagents and requires sample pre-treatment. If samples were acidified for storing, adjust the ph between 4 and 5 with 5 mol/l (5 N) Sodium hydroxide before test. Do not exceed ph 5, as manganese may precipitate. Interferences: Interfering Substance Calcium Chloride Iron Interference Level Greater than 700 mg/l Greater than 70,000 mg/l Greater than 5 mg/l Magnesium Greater than 100,000 mg/l Page 51

56 AC4P42 Molybdate / Molybdenum, Mercaptoacetic Acid Method, Powder Test Procedure mg/l MoO 4 / mg/l Mo 1. Load and run the AC4P42 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Molybdenum HR 1 F10 Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. 8. Add one Molybdenum HR 2 F10 Powder Pack straight from the foil to the same vial. 9. Close the vial tightly with the cap and swirl or invert several times to mix the contents. 10. Add one Molybdenum HR 3 F10 Powder Pack straight from the foil to the same vial. 11. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 12. Wait for a reaction period of 5 minutes Press the Measure Sample function key to display the result in mg/l Molybdate/Molybdenum. Filter turbid water samples using filter paper and funnel before analysis. Highly buffered water samples or extreme ph values should be adjusted to a ph of nearly 7 with 1 mol/l nitric acid or 1 mol/l sodium hydroxide. Concentrations above 10 mg/l Cu causes too high test values if the reaction time of 5 minutes is increased. So it is very important to perform the test procedure as described. Substances which may interfere when present in concentrations at: Aluminum 50 mg/l Chromium Iron Nickel Nitrite 1000 mg/l 50 mg/l 50 mg/l All Levels Page 52

57 ACR007 Nitrate as Nitrogen (N), Chromotropic Acid Method, Reaction Tube Test Procedure 1 30 mg/l N 1. Load and run the ACR007 method. 2. Open one white capped 16mm reaction vial (Reagent A) and add 1 ml of deionized water (this is the blank). 3. Open a second white capped 16mm reaction vial (Reagent A) and add 1 ml of sample (this is the sample). 4. Add the contents of one Nitrate Chromotropic Powder Pack straight from the foil to each vial. 5. Close the vials tightly with the caps and invert gently about 10 times to mix the contents. Some solids may not dissolve. Wipe the exteriors of the vials. 6. Wait for a reaction period of 5 minutes. 7. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. 8. Press the Measure Blank function key to measure the blank. 9. Open the sample chamber door. Remove the blank vial from the holder. 10. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l nitrate as N. Conversion: mg/l NO 3 = mg/l N x 4.43 Page 53

58 AC2046 Nitrite as Nitrogen (N), Diazotization (Azo) Method, Tablet Test Procedure mg/l N 1. Load and run the AC2046 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Nitrite LR Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved. Wipe the exterior of the vial. 8. Wait for a reaction period of 10 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l nitrite as N. The following ions can produce interferences since under the reaction conditions they cause precipitation: antimony (III), iron (III), lead, mercury (I), silver, chloroplatinate, metavanadate and bismuth. Copper (II) ions may cause lower test results as they accelerate the decomposition of the diazonium salt. It is unlikely in practice that these interfering ions will occur in such high concentrations that they cause significant reading errors. Conversion: mg/l NO 2 = mg/l N x 3.29 Page 54

59 AC4P46 Nitrite as Nitrogen (N), Low Range, Diazotization (Azo) Method, Powder Test Procedure mg/l N 1. Load and run the AC4P46 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Nitri 3 Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 8. Wait for a reaction period of 20 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l Nitrite as N. Interferences: o o o o Strong oxidizing and reducing substances interfere. Cupric and ferrous ions cause low results. Antimonous, auric, bismuth, chloroplatinate, ferric, lead, mercurous, metavanadate and silver ions interfere by causing precipitation. In samples with very high concentrations of Nitrate (> 100 mg/l N) a small amount of Nitrite will be found. Such high levels of Nitrate appear to undergo a slight amount of reduction to Nitrite, either spontaneously or during the reaction time of the test. Page 55

60 ACD004 Nitrogen, Total, Low Range, Persulfate Digestion Method, Digestion Tube Test Procedure mg/l N 1. Open two TN Hydroxide LR Digestion Vials and add one TN Persulfate Reagent Power Pack straight from the foil to each vial. Use a funnel to add the reagent. Wipe off any persulfate reagent that may get on the lid or the tube threads. 2. Add 2 ml of deionized water to the first digestion vial (this is the blank). 3. Add 2 ml of sample to the second digestion vial (this is the sample). 4. Close the vials tightly with the caps and shake the vials for at least 30 seconds to mix the contents. The reagent many not dissolve completely. 5. Heat the digestion vials for 30 minutes in the preheated reactor at a temperature of 100 C. 6. CAUTION: The vials will be hot. Remove the digestion vials from the reactor and allow them to cool to room temperature. 7. Open the cooled digestion vials and add one TN Reagent A Power Pack straight from the foil to each vial. Use a funnel to add the reagent. 8. Close the vials tightly with the caps and shake the vials for at least 15 seconds to mix the contents. 9. Wait for a reaction period of 3 minutes. 10. Open the digestion vials and add one TN Reagent B Power Pack straight from the foil to each vial. Use a funnel to add the reagent. 11. Close the vials tightly with the caps and shake the vials for at least 15 seconds to mix the contents. The reagent will not completely dissolve. 12. Wait for a reaction period of 2 minutes. 13. Open two TN Acid LR/HR (Reagent C) Vials and add 2 ml of the digested, treated blank to the first vial (this is the blank). 14. Add 2 ml of the digested, treated sample to the second vial (this is the sample). 15. Close the vials tightly with the caps and gently invert the vials at least 10 times to mix the contents. Hold the vial in a vertical position with the cap pointing up. Turn the vial upside-down. Wait for all of the solution to flow down to the cap. Return the vial to the upright position. Wait for all the solution to flow to the bottom of the vial. This process is one inversion; 10 inversions equal about 30 seconds. Wipe the exteriors of the vials. CAUTION: The vials will become warm during mixing. 16. Wait for a reaction period of 5 minutes. 17. Load and run the ACD004 method. 18. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. Page 56

61 19. Press the Measure Blank function key to measure the blank. 20. Open the sample chamber door. Remove the blank vial from the holder. 21. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 22. Press the Measure Sample function key to display the result in mg/l nitrogen. Appropriate safety precautions and a good lab technique should be used during the whole procedure. Volumes for samples and blank should always be metered by using 2 ml volumetric pipettes (class A). One blank is sufficient for each set of samples. After taking the blank measurement it is possible to measure several samples. It is very important to remove the vials from the reactor after exactly 30 minutes. Large quantities of nitrogen free, organic compounds which are included in some water samples may reduce the effectiveness of the digestion by reacting with the persulfate reagent. Samples which are well known to contents large quantities of organic compounds must be diluted and digestion and measurement must be repeated for checking the effectiveness of the digestion. Application: for water, wastewater and seawater. Interferences: Interfering substances that resulted in a concentration change of 10%: Bromide more than 60 mg/l and Chloride more than 1000 mg/l produce positive interferences. Page 57

62 ACD007 Nitrogen, Total, High Range, Persulfate Digestion Method, Digestion Tube Test Procedure mg/l N 1. Open two TN Hydroxide HR Digestion Vials and add one TN Persulfate Reagent Power Pack straight from the foil to each vial. Use a funnel to add the reagent. Wipe off any persulfate reagent that may get on the lid or the tube threads. 2. Add 0.5 ml of deionized water to the first digestion vial (this is the blank). 3. Add 0.5 ml of sample to the second digestion vial (this is the sample). 4. Close the vials tightly with the caps and shake the vials for at least 30 seconds to mix the contents. The reagent many not dissolve completely. 5. Heat the digestion vials for 30 minutes in the preheated reactor at a temperature of 100 C. 6. CAUTION: The vials will be hot. Remove the digestion vials from the reactor and allow them to cool to room temperature. 7. Open the cooled digestion vials and add one TN Reagent A Power Pack straight from the foil to each vial. Use a funnel to add the reagent. 8. Close the vials tightly with the caps and shake the vials for at least 15 seconds to mix the contents. 9. Wait for a reaction period of 3 minutes. 10. Open the digestion vials and add one TN Reagent B Power Pack straight from the foil to each vial. Use a funnel to add the reagent. 11. Close the vials tightly with the caps and shake the vials for at least 15 seconds to mix the contents. The reagent will not completely dissolve. 12. Wait for a reaction period of 2 minutes. 13. Open two TN Acid LR/HR (Reagent C) Vials and add 2 ml of the digested, treated blank to the first vial (this is the blank). 14. Add 2 ml of the digested, treated sample to the second vial (this is the sample). 15. Close the vials tightly with the caps and gently invert the vials at least 10 times to mix the contents. Hold the vial in a vertical position with the cap pointing up. Turn the vial upside-down. Wait for all of the solution to flow down to the cap. Return the vial to the upright position. Wait for all the solution to flow to the bottom of the vial. This process is one inversion; 10 inversions equal about 30 seconds. Wipe the exteriors of the vials. CAUTION: The vials will become warm during mixing. 16. Wait for a reaction period of 5 minutes. 17. Load and run the ACD007 method. 18. Place the blank vial into the holder in the sample chamber. Close the sample chamber door. Page 58

63 19. Press the Measure Blank function key to measure the blank. 20. Open the sample chamber door. Remove the blank vial from the holder. 21. Place the sample vial into the holder in the sample chamber. Close the sample chamber door. 22. Press the Measure Sample function key to display the result in mg/l nitrogen. Appropriate safety precautions and a good lab technique should be used during the whole procedure. Volumes for samples and blank should always be metered by using 2 ml volumetric pipettes (class A). One blank is sufficient for each set of samples. After taking the blank measurement it is possible to measure several samples. It is very important to remove the vials from the reactor after exactly 30 minutes. Large quantities of nitrogen free, organic compounds which are included in some water samples may reduce the effectiveness of the digestion by reacting with the persulfate reagent. Samples which are well known to contents large quantities of organic compounds must be diluted and digestion and measurement must be repeated for checking the effectiveness of the digestion. Application: for water, wastewater and seawater. Interferences: Interfering substances that resulted in a concentration change of 10%: Bromide more than 60 mg/l and Chloride more than 1000 mg/l produce positive interferences. Page 59

64 AC2048 Ozone, Indigo Blue, Tablet Test Procedure mg/l O 3 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of deionized water. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Rinse a clean beaker with deionized water. Add one Ozone Tablet straight from the foil to the beaker. Crush the tablet with a clean stir rod. Add exactly 20 ml of deionized water to the beaker. Carefully mix the solution using the stir rod until all particles are fully dissolved. 7. Empty and dry the vial and add the solution from the beaker to the 10 ml mark on the vial. 8. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Rgnt Blank function key to measure the reagent blank. 11. Open the sample chamber door and remove the vial from the sample chamber. 12. Rinse a clean beaker with the sample to be measured. Add one Ozone Tablet straight from the foil to the beaker. Crush the tablet with a clean stir rod. Add exactly 20 ml of sample to the beaker. Carefully mix the solution using the stir rod until all particles are fully dissolved. 13. Empty the vial, rinse the vial and cap several times and add the solution from the beaker to the 10 ml mark on the vial. 14. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 15. Place the vial into the holder in the sample chamber. Close the sample chamber door. 16. Press the Measure Sample function key to display the result in mg/l ozone. Reverse color methods use a reagent that, when prepared with samples, deceases in color as the concentration of the species being measured in the samples increases. Reverse color methods require the use of both a blank and a reagent blank. The blank is a clear solution (deionized water) with zero absorbance. The reagent blank is a mixture of the reagent and deionized water and provides a zero concentration point with the darkest color (highest absorbance). The color of samples prepared with the reagent will decrease as the concentration increases for this method. Page 60

65 Preparing the sample: When preparing the sample, the escape of ozone gases, i.e. by pipetting or shaking, must be avoided. The analysis must take place immediately after taking the sample. Strong alkaline or acidic water samples must be adjusted between ph 6 and ph 7 before the tablet is added (use 0.5 mol/l sulfuric acid or 1 mol/l sodium hydroxide). The malonic acid in the tablet prevents chlorine from interfering with the process. Bromine (or bromide oxidized by the ozone) interferes with the analysis. 1 mol HOBr is equivalent to 0.4 mol ozone. H 2 O 2 and organic peroxides react extremely slowly and the interference is therefore negligible. Fe(III) does not interfere. Mn(II) is oxidized by ozone and interferes with the analysis. Page 61

66 AC2001 ph, Phenol Red Method, Tablet Test Procedure ph 1. Load and run the AC2001 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Phenol Red Meter Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved. Wipe the exterior of the vial. 8. Place the vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Sample function key to display the result in ph units. For photometric determination of ph values only use Phenol Red Tablets in black printed foil pack and marked with Meter. Water samples with low values of alkalinity-m (below 35 mg/l CaCO 3 ) may give wrong ph readings. ph values below 6.5 and above 8.4 can produce results inside the measuring range. A plausibility test (ph meter) is recommended. The accuracy of the colorimetric determination of ph values depends on various boundary conditions (buffer capacity of the sample, salt contents etc.). Salt error: Correction of test results (average values) for samples with salt contents of: Indicator Salt Content Phenol Red 1 molar 2 molar 3 molar The values of Parson and Douglas (1926) are based on the use of Clark and Lubs buffers. 1 Mol NaCl = 58.4 g/l = 5.8 % Page 62

67 AC3001 ph, Phenol Red Method, Liquid Test Procedure ph 1. Load and run the AC3001 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add six drops of Phenol Red Solution to the vial. Add drops of the same size by holding the bottle vertically and squeezing slowly. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 8. Place the vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Sample function key to display the result in ph units. When testing chlorinated water the residual chlorine contents can influence the color reaction of the liquid reagent. This can be avoided (without interfering with the ph measurement) by adding a small crystal of sodium thiosulfate (Na 2 S 2 O 3 5 H 2 O) to the sample before adding the Phenol Red solution. Phenol Red tablets already contain thiosulfate. Due to differing drop sizes results can show a discrepancy in accuracy by comparison with tablets. This can be minimized by using a pipette (0.18 ml Phenol Red solution is equivalent to 6 drops). After use, replace the bottle cap securely. Store the Phenol Red solution in a cool, dry place ideally at between 6 C and 10 C. Page 63

68 AC2095 Phosphate, Ortho, Low Range, Phosphomolybdic Acid/Ascorbic acid Method, Tablet Test Procedure mg/l PO 4 1. Load and run the AC2095 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Phosphate No. 1 LR 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Add one Phosphate No. 2 LR Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 8. Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved. Wipe the exterior of the vial. 9. Wait for a reaction period of 10 minutes. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l ortho-phosphate. Only ortho-phosphate ions react. The tablets must be added in the correct sequence. The test sample should have a ph value between 6 and 7. Interferences: Higher concentrations of Cu, Ni, Cr (III), V (V) and W (VI) interfere due to their color. Silicates do not interfere (masked by citric acid in the tablets). Ortho-phosphate ions react with the reagent to form an intense blue color. Phosphate in organic and condensed inorganic forms (meta-, pyro- and polyphosphates) must be converted to ortho-phosphate ions before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms. Organically combined phosphates are converted to ortho-phosphate ions by heating with acid and persulfate. The amount of organically combined phosphates can be calculated: mg/l phosphate, organic = mg/l phosphate, total - mg/l phosphate, acid hydrolyzable Phosphate, ortho = Phosphorus, reactive Page 64

69 AC2096 Phosphate, Ortho, High Range, Vanadomolybdate Method, Tablet Test Procedure 1 80 mg/l PO 4 1. Load and run the AC2096 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Phosphate HR P1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Add one Phosphate HR P2 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 8. Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved. Wipe the exterior of the vial. 9. Wait for a reaction period of 10 minutes. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l ortho-phosphate. For samples under 5 mg/l PO 4 it is recommended to analyze the sample using the AC2095 method. Only ortho-phosphate ions react. Phosphate in organic and condensed inorganic forms (meta-, pyro- and polyphosphates) must be converted to ortho-phosphate ions before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms. Organically combined phosphates are converted to ortho-phosphate ions by heating with acid and persulfate. The amount of organically combined phosphates can be calculated: mg/l phosphate, organic = mg/l phosphate, total - mg/l phosphate, acid hydrolysable The ortho-phosphate ions react with the Vanadate-molybdate reagent under acid conditions to form a yellow colored product. Phosphate, ortho = Phosphorus, reactive Page 65

70 AC4P95 Phosphate, Ortho, Ascorbic Acid Method, Powder Test Procedure mg/l PO 4 1. Load and run the AC4P95 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Phosphate Rgt. F10 Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times for seconds to mix the contents. The powder will not dissolve completely. Wipe the exterior of the vial. 8. Wait for a reaction period of 2 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l ortho-phosphate. Ortho-phosphate ions react with the reagent to form an intense blue color. Phosphate in organic and condensed inorganic forms (meta-, pyro- and polyphosphates) must be converted to ortho-phosphate ions before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms. Organically combined phosphates are converted to ortho-phosphate ions by heating with acid and persulfate. The amount of organically combined phosphates can be calculated: mg/l phosphate, organic = mg/l phosphate, total - mg/l phosphate, acid hydrolysable Application: for water, wastewater and seawater. Highly buffered samples or samples with extreme ph values should be adjusted between ph 2 and ph 10 before analysis (with 1 mol/l Hydrochloric acid or 1 mol/l sodium hydroxide). Phosphate, ortho = Phosphorus, reactive Interferences: Large amounts of turbidity may cause inconsistent results. Interference Interference Level Interference Interference Level Aluminum greater than 200 mg/l Nickel greater than 300 mg/l Arsenate at any level Silica (Silicium dioxide) greater than 50 mg/l Chromium greater than 100 mg/l Silicate greater than 10 mg/l Copper greater than 10 mg/l Sulfide at any level Iron greater than 100 mg/l Zinc greater than 80 mg/l Page 66

71 ACD095 Phosphate as Phosphorous (P), Total, Persulfate Digestion/Ascorbic Acid Method, Digestion Tube Test Procedure mg/l P 1. Open one white capped 16mm PO4-P Acid Reagent Digestion Tube and add 5 ml of sample. 2. Add one Potassium Persulfate F10 Power Pack straight from the foil to the vial. Use a funnel to add the reagent. 3. Close the vial tightly with the cap and invert the vial several times to mix the contents. 4. Heat the vial for 30 minutes in the preheated reactor at a temperature of 100 C. 5. CAUTION: The vials will be hot. Remove the vial from the reactor and allow it to cool to room temperature. 6. Open the cooled digestion vial and add 2 ml of 1.54 N Sodium Hydroxide Solution to the vial. 7. Close the vial tightly with the cap and gently invert the vial several times to mix the contents. Wipe the exterior of the vial. 8. Load and run the ACD095 method. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Blank function key to measure the blank. 11. Open the sample chamber door. Remove the vial from the holder. 12. Add one Phosphate Rgt. F10 Power Pack straight from the foil to the vial. Use a funnel to add the reagent. 13. Close the vial tightly with the cap and swirl the vial for seconds to mix the contents. The reagent will not completely dissolve. Wipe the exterior of the vial. 14. Wait for a reaction period of 2 minutes. 15. Place the vial into the holder in the sample chamber. Close the sample chamber door. 16. Press the Measure Sample function key to display the result in mg/l total phosphate. Appropriate safety precautions and good lab technique should be used during the whole procedure. Ortho-phosphate ions react with the reagent to form an intense blue color. Phosphate in organic and condensed inorganic forms (meta-, pyro- and polyphosphates) must be converted to ortho-phosphate ions before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms. Organically combined phosphates are converted to ortho-phosphate ions by heating with acid and persulfate. The amount of organically combined phosphates can be calculated: mg/l phosphate, organic = mg/l phosphate, total - mg/l phosphate, acid hydrolysable Page 67

72 Application: for water, wastewater and seawater. Highly buffered samples or samples with extreme ph values should be adjusted between ph 2 and ph 10 before analysis (with 1 mol/l Hydrochloric acid or 1 mol/l sodium hydroxide). Phosphate, ortho = Phosphorus, reactive Interferences: Large amounts of turbidity may cause inconsistent results. Interfering Substance Aluminum Arsenate Chromium Copper Iron Nickel Silica (Silicium dioxide) Silicate Sulfide Zinc Interference Level greater than 200 mg/l at any level greater than 100 mg/l greater than 10 mg/l greater than 100 mg/l greater than 300 mg/l greater than 50 mg/l greater than 10 mg/l at any level greater than 80 mg/l Page 68

73 ACD095AH Phosphate as Phosphorous (P), Acid Hydrolyzable, Acid Digestion/Ascorbic Acid Method, Digestion Tube Test Procedure mg/l P 1. Open one white capped 16mm PO4-P Acid Reagent Digestion Tube and add 5 ml of sample. 2. Close the vial tightly with the cap and gently invert the vial several times to mix the contents. 3. Heat the vial for 30 minutes in the preheated reactor at a temperature of 100 C. 4. CAUTION: The vials will be hot. Remove the vial from the reactor and allow it to cool to room temperature. 5. Open the cooled digestion vial and add 2 ml of 1.00 N Sodium Hydroxide Solution to the vial. 6. Close the vial tightly with the cap and gently invert the vial several times to mix the contents. Wipe the exterior of the vial. 7. Load and run the ACD095AH method. 8. Place the vial into the holder in the sample chamber. Close the sample chamber door. 9. Press the Measure Blank function key to measure the blank. 10. Open the sample chamber door. Remove the vial from the holder. 11. Add one Phosphate Rgt. F10 Power Pack straight from the foil to the vial. Use a funnel to add the reagent. 12. Close the vial tightly with the cap and swirl the vial for seconds to mix the contents. The reagent will not completely dissolve. Wipe the exterior of the vial. 13. Wait for a reaction period of 2 minutes. 14. Place the vial into the holder in the sample chamber. Close the sample chamber door. 15. Press the Measure Sample function key to display the result in mg/l acid hydrolysable phosphate. Appropriate safety precautions and good lab technique should be used during the whole procedure. Ortho-phosphate ions react with the reagent to form an intense blue color. Phosphate in organic and condensed inorganic forms (meta-, pyro- and polyphosphates) must be converted to ortho-phosphate ions before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms. Organically combined phosphates are converted to ortho-phosphate ions by heating with acid and persulfate. The amount of organically combined phosphates can be calculated: mg/l phosphate, organic = mg/l phosphate, total - mg/l phosphate, acid hydrolysable Application: for water, wastewater and seawater. Page 69

74 Highly buffered samples or samples with extreme ph values should be adjusted between ph 2 and ph 10 before analysis (with 1 mol/l Hydrochloric acid or 1 mol/l sodium hydroxide).\ Phosphate, ortho = Phosphorus, reactive Interferences: Large amounts of turbidity may cause inconsistent results. Interfering Substance Aluminum Arsenate Chromium Copper Iron Nickel Silica (Silicium dioxide) Silicate Sulfide Zinc Interference Level greater than 200 mg/l at any level greater than 100 mg/l greater than 10 mg/l greater than 100 mg/l greater than 300 mg/l greater than 50 mg/l greater than 10 mg/l at any level greater than 80 mg/l Page 70

75 ACR095 Phosphate, Ortho, Ascorbic Acid Method, Reaction Tube Test Procedure mg/l PO 4 1. Load and run the ACR095 method. 2. Open one white capped 16mm PO4-P Dilution Tube and add 5 ml of sample. Wipe the exterior of the vial. 5. Open the sample chamber door. Remove the vial from the holder. 6. Add one Phosphate Rgt. F10 Power Pack straight from the foil to the vial. Use a funnel to add the reagent. 7. Close the vial tightly with the cap and swirl the vial for seconds to mix the contents. The reagent will not completely dissolve. Wipe the exterior of the vial. 8. Wait for a reaction period of 2 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l ortho-phosphate. Ortho-phosphate ions react with the reagent to form an intense blue color. Phosphate in organic and condensed inorganic forms (meta-, pyro- and polyphosphates) must be converted to ortho-phosphate ions before analysis. Pretreatment of the sample with acid and heat provides the conditions for hydrolysis of the condensed inorganic forms. Organically combined phosphates are converted to ortho-phosphate ions by heating with acid and persulfate. The amount of organically combined phosphates can be calculated: mg/l phosphate, organic = mg/l phosphate, total - mg/l phosphate, acid hydrolysable Application: for water, wastewater and seawater. Highly buffered samples or samples with extreme ph values should be adjusted between ph 2 and ph 10 before analysis (with 1 mol/l Hydrochloric acid or 1 mol/l sodium hydroxide). Phosphate, ortho = Phosphorus, reactive Interferences: Large amounts of turbidity may cause inconsistent results. Interference Interference Level Interference Interference Level Aluminum greater than 200 mg/l Nickel greater than 300 mg/l Arsenate at any level Silica (Silicium dioxide) greater than 50 mg/l Chromium greater than 100 mg/l Silicate greater than 10 mg/l Copper greater than 10 mg/l Sulfide at any level Iron greater than 100 mg/l Zinc greater than 80 mg/l Page 71

76 AC2060 Silica, Silicomolybdate Method, Tablet Test Procedure mg/l SiO 2 1. Load and run the AC2060 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Silica No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. 8. Wait for a reaction period of 5 minutes. 9. Add one Silica No. 2 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 10. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 11. Wait for a reaction period of 1 minute. 12. Place the vial into the holder in the sample chamber. Close the sample chamber door. 13. Press the Measure Sample function key to display the result in mg/l silica. The tablets must be added in the correct sequence. Page 72

77 AC2061 Silica, Silicomolybdate Method with Phosphate Removal, Tablet Test Procedure mg/l SiO 2 1. Load and run the AC2061 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Silica No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. 8. Wait for a reaction period of 5 minutes. 9. Add one Silica PR Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 10. Add one Silica No. 2 Tablet straight from the foil to the same vial. Crush the tablet with a clean stir rod. 11. Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved. Wipe the exterior of the vial. 12. Wait for a reaction period of 1 minute Press the Measure Sample function key to display the result in mg/l silica. The tablets must be added in the correct sequence. Phosphate ions do not interfere under the given reaction conditions. If phosphate is known to be absent, the addition of the Silica PR Tablet may be omitted. Page 73

78 AC4P60 Silica, High Range, Silicomolybdate Method, Powder Test Procedure 1 90 mg/l SiO 2 1. Load and run the AC4P60 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Temperature of the sample should be 15 C to 25 C. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Silica HR Molybdate F10 Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. 8. Add one Silica HR Acid Rgt. F10 Powder Pack straight from the foil to the same vial. If silica or phosphate is present a yellow color will develop. 9. Close the vial tightly with the cap and swirl or invert several times to mix the contents. 10. Wait for a reaction period of 10 minutes. 11. Add one Silica Citric Acid F10 Powder Pack straight from the foil to the same vial. In this step, any yellow color due to phosphate is removed. 12. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 13. Wait for a reaction period of 2 minutes. 14. Place the vial into the holder in the sample chamber. Close the sample chamber door. 15. Press the Measure Sample function key to display the result in mg/l silica. Interferences: Substance Interference Iron Large amounts interfere Phosphate Does not interfere at concentrations less than 50 mg/l PO 4 At 60 mg/l PO 4 the interference is approximately 2% At 75 mg/l PO 4 the interference is approximately 11 % Sulfide Interferes at all levels Occasionally water samples contain forms of silica which reacts very slowly with molybdate. The nature of these forms is not known. Page 74

79 A pre-treatment with sodium hydrogen carbonate and then with sulfuric acid will make these forms reactive to molybdate (pre-treatment is given in Standard Methods for the Examination of Water and Wastewater under Silica Digestion with Sodium Bicarbonate ). Page 75

80 AC4P82 Sulfate, Barium Sulfate/Turbidity Method, Powder Test Procedure mg/l SO 4 1. Load and run the AC4P82 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Sulpha 4/F10 Powder Pack straight from the foil to the vial. 7. Close the vial tightly with the cap and swirl or invert several times to mix the contents. Wipe the exterior of the vial. 8. Wait for a reaction period of 5 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Sample function key to display the result in mg/l sulfate. If sulfate ions are present a cloudy solution will appear. Page 76

81 AC2016 Sulfide, Methylene Blue Method, Tablet Test Procedure mg/l S 1. Load and run the AC2016 method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of sample. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Open the sample chamber door and remove the vial from the sample chamber. 6. Add one Sulfide No. 1 Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Add one Sulfide No. 2 Tablet straight from the foil to the same vial. Crush the tablet with a clean stir rod. 8. Close the vial tightly with the cap and swirl or invert several times until the tablets are dissolved. Wipe the exterior of the vial. 9. Wait for a reaction period of 10 minutes. 10. Place the vial into the holder in the sample chamber. Close the sample chamber door. 11. Press the Measure Sample function key to display the result in mg/l sulfide. The tablets must be added in the correct sequence. Chlorine and other oxidizing agents which react with DPD do not interfere with the test. To avoid loss of sulfide collect the sample carefully with a minimum of aeration. It is essential to test the sample immediately after collection. The sample temperature should be 20 C. A different temperature can lead to higher or lower results. Page 77

82 AC2065 Zinc, Zincon Method, Tablet Test Procedure mg/l Zn 1. Load and run the AC method. 2. Fill a clean AQUAfast 24mm round vial, Cat. No. AC2V24, with 10 ml of deionized water. Close the vial tightly with the cap. Wipe the exterior of the vial. 5. Empty and dry the vial and then fill the vial with 10 ml of sample. 6. Add one Copper / Zinc LR Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 7. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 8. Wait for a reaction period of 5 minutes. 9. Place the vial into the holder in the sample chamber. Close the sample chamber door. 10. Press the Measure Rgnt Blank function key to measure the reagent blank. 11. Open the sample chamber door and remove the vial from the sample chamber. 12. Add one EDTA Tablet straight from the foil to the vial. Crush the tablet with a clean stir rod. 13. Close the vial tightly with the cap and swirl or invert several times until the tablet is dissolved. Wipe the exterior of the vial. 14. Place the vial into the holder in the sample chamber. Close the sample chamber door. 15. Press the Measure Sample function key to display the result in mg/l zinc. Reverse color methods use a reagent that, when prepared with samples, deceases in color as the concentration of the species being measured in the samples increases. Reverse color methods require the use of both a blank and a reagent blank. The blank is a clear solution (deionized water) with zero absorbance. The reagent blank is a mixture of the reagent and sample (with no EDTA reagent) and provides a zero concentration point with the darkest color (highest absorbance). The color of samples prepared with the EDTA reagent will decrease as the concentration increases for this method. Measuring the reagent blank needs to be done with each sample analysis. The tablets must be added in the correct sequence. In the case of high levels of residual chlorine, perform the analysis with a dechlorinated water sample. To dechlorinate add one Dechlor Tablet to the water sample in step 2. Crush and mix to dissolve the tablet. Then add the Copper / Zinc LR Tablet (step 3) and continue with the test procedure as described above. Page 78

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